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UNIVERSITI PUTRA MALAYSIA PARALLEL EVOLUTION OF MICROSTRUCTURE, PHYSICAL PROPERTIES AND THEIR RELATIONSHIPS IN Co0.5Zn0.5Fe2O4 CERAMICS MUHAMMAD MISBAH BIN MUHAMAD ZULKIMI ITMA 2013 13

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UNIVERSITI PUTRA MALAYSIA

PARALLEL EVOLUTION OF MICROSTRUCTURE, PHYSICAL PROPERTIES AND THEIR RELATIONSHIPS IN Co0.5Zn0.5Fe2O4

CERAMICS

MUHAMMAD MISBAH BIN MUHAMAD ZULKIMI

ITMA 2013 13

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PARALLEL EVOLUTION OF

MICROSTRUCTURE, PHYSICAL PROPERTIES

AND THEIR RELATIONSHIPS IN Co0.5Zn0.5Fe2O4

CERAMICS

MUHAMMAD MISBAH BIN MUHAMAD ZULKIMI

MASTER OF SCIENCE

UNIVERSITI PUTRA MALAYSIA

2013

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PARALLEL EVOLUTION OF MICROSTRUCTURE, PHYSICAL

PROPERTIES AND THEIR RELATIONSHIPS IN Co0.5Zn0.5Fe2O4 CERAMICS

By

MUHAMMAD MISBAH BIN MUHAMAD ZULKIMI

Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia, in

Fulfilment of the Requirements for the Degree of Master of Science

November 2013

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All material contained within the thesis, including without limitation text, logos, icons,

photographs and all other artwork, is copyright material of Universiti Putra Malaysia

unless otherwise stated. Use may be made of any material contained within the thesis

for non-commercial purposes from the copyright holder. Commercial use of material

may only be made with the express, prior, written permission of Universiti Putra

Malaysia.

Copyright © Universiti Putra Malaysia

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In appreciation of their love and sacrifices, this thesis is dedicated to Parents

MUHAMAD ZULKIMI AWANG and SUYATI ABD RAZAK.

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Abstract of thesis presented to the Senate of Universiti Putra Malaysia in fulfillment of

the requirement for the degree of Master of Science

PARALLEL EVOLUTION OF MICROSTRUCTURE, PHYSICAL

PROPERTIES AND THEIR RELATIONSHIPS IN Co0.5Zn0.5Fe2O4 CERAMICS

By

MUHAMMAD MISBAH BIN MUHAMAD ZULKIMI

November 2013

Chairman: Associate Professor Mansor Hashim, PhD

Institute: Institute of Advanced Technology

For more than eight past decades, the ferrite research literature has only very

superficially dealt with the question of how the evolving microstructure of a ferrite

material relates to its accompanying, resultant magnetic properties. The literature has

only covered in great detail the answers for the case of ferrite materials obtained from

final sintering. Thus, this work is a fresh attempt to critically track the evolution of

magnetic properties parallel to the microstructural changes in bulk Co0.5Zn0.5Fe2O4

samples and to relate the properties to the changes wherever possible.

In this study, high energy ball milling (HEBM) was used to prepare Co0.5Zn0.5Fe2O4

nanoparticles with sintering temperatures from 500 oC to 1350

oC and with a 50

oC

increment. Physical characteristics of the as-prepared and sintered samples were studied

using X-ray diffraction (XRD), scanning transmission electron microscopy (STEM) and

Field Emission Scanning Electron Microscope (FESEM); characterization of magnetic

properties was carried out by using An Agilent Model 4291B impedance/material

analyser in the frequency range of 1 MHz to 1.0 GHz which was used to measure the

permeability and the loss factor. The magnetic properties of the samples were

investigated using a MATS-2010SD Static Hysteresisgraph.

The XRD results confirm that Cobalt zinc ferrite cannot be formed directly through

milling alone, but heat treatment is necessary. After sintering at 550 oC, the cobalt zinc

ferrite phase was obtained earliest at this temperature with an average grain size in the

nanometric range (0.089µm). The microstructure studies of Co0.5Zn0.5Fe2O4 showed that

the grain size increased, density was increased and porosity was decreased as the

sintering temperature increased. The parallel evolution of hysteresis parameters with

microstructural properties for sintered samples was studied. The saturation induction,

Bs, increased with the enhancement grain size. The highest saturation induction value

for sintered samples is 1486.00 G. The coercivity value was increased with increasing

grain size and reached a maximum value (24.93 Oe) before dropping with further

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increasing grain size. The permeability and loss factor values were observed and can be

classified into three different groups with the utilization the similar B-H hysteresis loop

results: weak ferromagnetic (first group), moderate magnetic (second group) and strong

ferromagnetic (third group) behavior. The resistivity value of the sample under

investigation had semiconductor behavior. The Curie temperature varied slightly for the

samples due to stoichiometric changes allocated with zinc loss.

Finally, after analysing the results and the observations of the work mentioned above, it

is strongly believed that there are three factors found to sensitively influence the

samples content of ordered magnetism –their ferrite-phase crystallinity degree, the

number of grains above the critical grain size and large enough grains for domain wall

accomodation. This research work has shed new light on the microstructure-magnetic

properties evolution in ferrites.

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Abstrak tesis yang dikemukakan kepada senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk ijazah Master Sains

EVOLUSI SEIRING SIFAT-SIFAT MORFOLOGI, FIZIKAL DAN

HUBUNGANNYA DALAM SERAMIK Co0.5Zn0.5Fe2O4

Oleh

MUHAMMAD MISBAH BIN MUHAMAD ZULKIMI

November 2013

Pengerusi: Profesor Madya Mansor Hashim, PhD

Institut: Institut Teknologi Maju

Sejak daripada lapan dekad yang lampau, kajian penyelidikan ferit hanya menangani

persoalan bagaimana sesuatu mikrostruktur ferit yang sedang mengalami evolusi berkait

dengan sifat magnet yang terhasil seiring dengannya dengan tidak begitu mendalam.

Maka projek ini adalah cubaan terbaru untuk mencerap secara kritikal evolusi pencirian

magnet seiring dengan perubahan mikrostruktur bagi sampel Co0.5Zn0.5Fe2O4.

Dalam kajian ini, pengisaran bola bertenaga tinggi (HEBM) telah digunakan untuk

menyediakan Co0.5Zn0.5Fe2O4 bersaiz nano dengan suhu pensinteran bermula dari 500 oC 1350

oC dan kenaikan 50

oC. Ciri-ciri fizikal sampel dikaji menggunakan pembiasan

sinar-X (XRD), mikroskop pengimbas elektron (STEM) dan mikroskop pengimbas

medan elekron (FESEM) dan pencirian sifat magnet dengan menggunakan Agilent

Model 4291B Rangkaian / Spectrum analyzer dalam julat frekuensi 1 MHz hingga 1.0

GHz telah digunakan untuk mengukur ketelapan dan faktor kehilangannya. Sifat-sifat

magnet sampel telah dikaji dengan menggunakan Hysteresisgraph statik Mats-2010SD.

Keputusan XRD mengesahkan bahawa Cobalt zink ferit tidak boleh dibentuk secara

langsung melalui pengisaran sahaja, tetapi rawatan haba diperlukan. Selepas persinteran

sampel pada 550 oC, fasa kobalt zink ferit diperolehi pada suhu ini dengan saiz purata

mikrostruktur dalam lingkungan nano (0.089 μm). Kajian mikrostruktur Co0.5Zn0.5Fe2O4

menunjukkan bahawa saiz butiran meningkat bersama dengan peningkatan nilai

ketumpatan dan liang-liang udara menurun apabila suhu pensinteran meningkat. Evolusi

selari parameter histerisis dengan ciri-ciri mikrostruktur untuk sampel tersinter telah

dikaji. Induksi tepu, Bs, meningkat dengan peningkatan saiz butiran. Nilai tertinggi

induksi tepu untuk sampel tersinter adalah 1486.00 G. Nilai daya paksa (Hc) meningkat

dengan peningkatan saiz butiran dan mencapai nilai maksimum 24.93 Oe sebelum ia

menurun dengan peningkatan saiz butiran. Ketelapan dan nilai-nilai faktor kehilangan

diperhatikan dan boleh dikelaskan kepada tiga kumpulan yang berbeza dengan

penggunaan BH keputusan gelung histerisis yang sama iaitu: feromagnet lemah

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(kumpulan pertama), magnet sederhana (kumpulan kedua) dan tingkah laku feromagnet

yang tinggi (kumpulan ketiga). Nilai kerintangan sampel yang dikaji pula mempunyai

sifat semikonduktor. Suhu Curie berubah sedikit untuk sampel yang disebabkan oleh

perubahan stoikiometri yang berlaku kerana kehilangan zink.

Akhir sekali, selepas menganalisis keputusan dan pemerhatian kerja yang dilakukan,

diyakini bahawa terdapat tiga faktor yang secara sensitif mempengaruhi kandungan

kemagnetan bertertib sampel iaitu darjah fasa kehabluran, jumlah butiran melepasi saiz

kritikal butiran dan butiran yang cukup besar untuk penempatan dinding domain. Kajian

penyelidikan ini telah menyumbangkan pengetahuan baharu tentang terhadap evolusi

mikrostruktur-sifat magnet dalam bahan ferit.

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ACKNOWLEDGEMENTS

It is neither my strength nor my wisdom, but Allah‟s mercies that made this work a

success, thus, I glorify Him. May all praises and salutations of the Lord be upon the

Messenger of Allah and upon his Family and Companions, and those who are guided by

the light of his „sunnah‟ till the Day of Judgment.

Countless of people contribute to this thesis; mentors and /or supervisors, family,

friends and even some strangers have set off trains of thought and spark ideas or

understandings. This means that, by mentioning names, I would be omitting someone.

Never the less, my unreserved appreciation goes to my able supervisor Associate

Professor Dr. Mansor Hashim for his guidance and suggestions, without which, this

work would not have been a success. This thesis is, but a fraction of evidence reflecting

his vast insight into magnetism and magnetic materials. I am highly indebted and

eternally grateful. To my co-supervisors, Dr.Raba‟ah Syahidah Azis, I thank to her for

keeping me right on track and contributions would forever remain indelible in my

memories.

To my colleagues in the magnetic materials research group.I appreciate the memorable

interactions that we had from where I drew my strength, thank you very much for

lighting my path; „please lets keep the ball rolling, and bit faster, if possible‟. To my

numerous friends, I say thanks for everything.

In measuring the characteristics of my samples, Institute of Advance Technology

(ITMA,UPM) and Physics Dept. UPM (XRD) are highly acknowledged.

My particular thanks are owed to my beloved family who were always there when in

need. Thank you for all you support. May ALLAH s.w.t will always bless you

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I certify that a Thesis Examination Committee has met on 19 November 2013 to

conduct the final examination of Muhammad Misbah bin Muhamad Zulkimi on his

thesis entitled “Parallel Evolution of Microstructure, Physical Properties, and Their

Relationships in Co0.5Zn0.5Fe2O4 Ceramics” in accordance with the Universities and

University Colleges Act 1971 and the Constitution of the Universiti Putra Malaysia

[P.U.(A) 106] 15 March 1998. The Committee recommends that the student be awarded

the master science

Members of the Thesis Examination Committee were as follows:

Zaidan bin Abdul Wahab, PhD Associate Professor

Faculty of Science

Universiti Putra Malaysia

(Chairman)

Jumiah binti Hassan, PhD Associate Professor

Faculty of Science

Universiti Putra Malaysia

(Internal Examiner)

Khamirul Amin bin Matori, PhD Senior Lecturer

Faculty of Science

Universiti Putra Malaysia

(Internal Examiner)

Ahmad Fauzi Mohd Noor, PhD Professor

Universiti Sains Malaysia

Malaysia

(External Examiner)

_________________________________

NORITAH OMAR, PhD

Associate Professor and Deputy Dean

School of Graduate Studies

Universiti Putra Malaysia

Date: 21 January 2014

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This thesis was submitted to the Senate of Universiti Putra Malaysia and has been

accepted as fulfillment of the requirement for the degree of Master of Science. The

members of the Supervisory Committee are as follows:

Mansor Hashim, PhD

Associate Professor

Institute of Advance Technology

Universiti Putra Malaysia

(Chairman)

Raba’ah Syahidah Azis, PhD

Senior Lecturer

Faculty of Science

Universiti Putra Malaysia

(Member)

BUJANG BIN KIM HUAT, PhD Professor and Dean

School of Graduate Studies

Universiti Putra Malaysia

Date:

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DECLARATION

Declaration by graduate student

I hereby confirm that:

this thesis is my original work;

quotations, illustrations and citations have been duly referenced;

this thesis has not been submitted previously or concurrently for any other

degree at any other institutions;

intellectual property from the thesis and copyright of thesis are fully-owned by

Universiti Putra Malaysia, as according to the Universiti Putra Malaysia

(Research) Rules 2012;

written permission must be obtained from supervisor and the office of Deputy

Vice-Chancellor (Research and Innovation) before thesis is published (in the

form of written, printed or in electronic form) including books, journals,

modules, proceedings, popular writings, seminar papers, manuscripts, posters,

reports, lecture notes, learning modules or any other materials as stated in the

Universiti Putra Malaysia (Research) Rules 2012;

there is no plagiarism or data falsification/fabrication in the thesis, and scholarly

integrity is upheld as according to the Universiti Putra Malaysia (Graduate

Studies) Rules 2003 (Revision 2012-2013) and the Universiti Putra Malaysia

(Research) Rules 2012. The thesis has undergone plagiarism detection software.

Signature: _______________________ Date: __19 November 2013

Name and Matric No.: Muhammad Misbah Bin Muhamad Zulkimi (GS31274)

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Declaration by Members of Supervisory Committee

This is to confirm that:

the research conducted and the writing of this thesis was under our

supervision;

supervision responsibilities as stated in the Universiti Putra Malaysia

(Graduate Studies) Rules 2003 (Revision 2012-2013) are adhered to.

Signature: _____________________ Signature: ________________________

Name of

Chairman of

Supervisory

Committee:

Mansor Hashim, PhD

Name of

Member of

Supervisory

Committee:

Raba‟ah Syahidah Azis, PhD

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TABLE OF CONTENTS

Page

DEDICATION i

ABSTRACT ii

ABSTRAK iv

ACKNOWLEDGEMENTS vi

APPROVAL vii

DECLARATION ix

LIST OF TABLES xiv

LIST OF FIGURES xv

LIST OF ABBREVIATIONS xvii

CHAPTER

1. INTRODUCTION 1

1.1 Background of the Study 1

1.2 Ferrite Materials 1

1.3 Problem Statement 2

1.4 Objectives 2

1.5 Thesis Outline

3

2. LITERATURE REVIEW AND THEORY

4

2.1 Introduction 4

2.2 Preparation of spinel ferrite 4

2.2.1 Wet chemical method 4

2.2.2 Physical method 6

2.3 Structure of ferrite 7

2.4 Fundamentals of Magnetism 8

2.5 Classification of Magnetic Materials 8

2.6 Magnetic properties of ferrites 9

2.6.1 Intrinsic Properties 10

2.6.1.1 Saturation Magnetization 10

2.6.1.2 Curie Temperature 10

2.6.2 Extrinsic Properties 10

2.6.2.1 Domains Walls 10

2.6.2.2 Grain Size 11

2.6.2.3 Hysteresis loop 11

2.6.2.4 Permeability, µ‟ 12

2.6.2.5 Magnetic losses 13

2.6.2.6 Resistivity 14

2.7 Mechanical Alloying 14

2.7.1 Mechanism of mechanical alloying

15

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3. MATERIALS AND METHODS 17

3.0 Introduction 17

3.1 Research Design 17

3.2 Raw materials and preparations of nanoparticles 18

3.2.1 Chemical formula and weighing of constituent

powder

18

3.2.2 High Energy Ball Milling (HEBM) and toroidal

preparation

18

3.2.3Heat treatment (sintering) 19

3.3 Material characterization measurements 21

3.3.1 X-Ray Diffraction (XRD) 21

3.3.2 Scanning Transmission Electron Microscope

(STEM)

22

3.3.3 Field Emission Scanning Electron Microscope

(FESEM)

22

3.3.4 BH Hysteresis graph Measurement 23

3.3.5 Complex Permeability 23

3.3.6 Material Density Measurement 24

3.3.7 Resistivity Measurement 24

3.3.8 Curie Temperature 26

4. RESULTS AND DISCUSSION 27

4.1 Introduction 27

4.2 Microstructure-related analysis 27

4.2.1 Particle size analysis 27

4.2.2 Phase analysis 28

4.2.3 Microstructure Properties 31

4.2.3.1 Grain size distribution

4.2.3.2 Density and Porosity

4.2.3.3 Activation Energy

34

35

36

4.3 Magnetic Properties 38

4.3.1 B-H Hysteresis Loop 38

4.3.2 Complex permeability 43

4.3.2.1 Real permeability, µ‟ 43

4.3.2.2 Loss Factor, µ” 46

4.3.3 Temperature dependent Resistivity 50

4.3.4 Curie Temperature 53

4.4 Summary

54

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5.

CONCLUSIONS AND SUGGESTIONS 57

5.1 Conclusions 57

5.2 Suggestions 57

BIBLIOGRAPHY

APPENDIX

BIODATA OF STUDENT

LIST OF PUBLICATIONS,CONFERENCES AND WORKSHOP

58

62

63

64

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LIST OF TABLES

Table Page

2.1 Descriptions of orientations of the magnetic moment in

materials help to identify different forms of magnetism in

nature

9

4.1 Theoretical Density, Measured Density, Porosity and

Average Grain Size for cobalt zinc ferrite.

36

4.2 The Activation Energy for sintered sample of cobalt zinc

ferrite

38

4.3 Saturation Induction, Bs, and Coercivity, Hc, of sintered

sample

42

4.4 Summary of the initial permeability and loss factor of

sintered sample of Co0.5Zn0.5Fe2O4

49

4.5 Curie temperature of Co0.5Zn0.5Fe2O4 for samples sintered

800 oC to 1350

oC different sintering temperature

54

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LIST OF FIGURES

Figure Page

2.1 Schematic of partial unit cell of spinel ferrite structure.

7

2.2 Typical hysteresis loop of ferrite.

12

2.3 Stages of mechanical alloying process. 16

3.1 Flowchart for the preparation and characterization of

morphological and magnetic properties of the

Co0.5Zn0.5Fe2O4

20

3.2 XRD machine

21

3.3 FEI NOVA NanoSEM 230 machine

22

3.4 MATS-2010SD Static Hysteresisgraph

23

3.5 Agilent Impedance Analyzer Instrument 4291B

24

3.6 Temperature dependence Resistivity measurement set-up

25

3.7 Schematic diagram for Temperature dependence Resistivity

measurement.

26

3.8 Curie temperature measurement set-up

26

4.1 STEM image of the as-milled Co0.5Zn0.5Fe2O4, (b) grain

distribution of the as-milled Co0.5Zn0.5Fe2O4.

27

4.2 XRD pattern (a) for cobalt zinc ferrite sintered at 500 oC to

800 oC, (b) sintered at 850

oC to 1350

oC.

29

4.3 FESEM micrograph for cobalt zinc ferrite sintered samples

32

4.4 Grain size distribution for cobalt zinc ferrite sintered samples

34

4.5 Plots of log D versus the reciprocal of absolute temperature

(1/T)

38

4.6(a) B-H Hysteresis loop for the sintered samples. 40

4.6(b) Three B-H Hysteresis shape groups for sintered sample for:

(1) First group, (2) second group, and (3) third group

41

4.6(c) Coercivity versus average grain size for sintered samples

42

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4.7(a) Graph of real permeability, μ‟against frequency for sintered

sample at 500 oC to 1350

oC.

44

4.7(b) Three real permebility shape groups for sintered sample for:

(1) first group, (2) second group, and (3) third group

45

4.8(a) Graph of loss factor,μ” against frequency for sintered sample at

500 oC to 1350

oC.

47

4.8(b) Three loss Factor shape groups for sintered sample for:

(1) first group, (2) second group, and (3) third group

48

4.9 The temperature dependence of electrical resistivity for sintered

sample

51

4.10 The temperature dependence of electrical resistivity for sintered

sample: (a) first part, and (b) second part

52

4.11 Curie temperature for samples sintered 800 oC to 1350

oC at

different sintering temperature

53

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LIST OF ABBREVIATIONS

XRD X-ray diffraction

STEM Scanning Transmission Electron Microscopy

HEBM High Energy Ball Milling

kHz kilohertz

MHz megahertz

GHz gigahertz

wt % Weight percent

hkl Miller indices

ICDD Joint Committee on Power Diffraction Standard

BPR Ball-to-powder weight ratio

MA Mechanical alloying

a.u Arbitrary unit

H Magnetic field strength

HC Coercivity

M Mass magnetization

BS Saturation induction

θC Curie temperature

2θ 2 theta degree

µm microns

µ‟ Real permeability

µ” Loss factor

Ms Saturation magnetization

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CHAPTER 1

INTRODUCTION

1.1 Background of the study

Microstructure similar to any single-phase polycrystalline ceramic, complex systems

of magnetic oxide consisting of crystals pores and grain boundaries are called

polycrystalline ferrites. For these materials, their microstructure is strongly affected

by few factors such as the calcination temperature, quality raw materials and the

sintering temperature regime.

In most cases, the grains, the pore size, the porosity, the density, intra-granular and

inter granular distribution of pores and grains are the parameters of microstructure.

The quantity, size, shape and distribution of both crystal grains and pores of a ferrite

are influenced by different techniques and preparation conditions.

The magnetic properties of these ferrites are determined and strongly influenced by

the chemical composition, the crystal structure and the microstructural parameters

such as grain size, grain size distribution, porosity, etc. obtained at a particular

sintering temperature. Unfortunately, for several decades, studies of the relationship

between magnetic properties and morphological properties have been focusing only

on the product of the final sintering temperature. These studies abandoned any

detailed tracking of the parallel evolutions of morphology and magnetic properties in

the 1 nm-to-1µm grain materials, which could have been observed by the early ferrite

researchers using wet-chemistry synthesis methods.

The question in the recent work is whether we are able to provide a good explanation

of the evolution relationships between magnetic properties and morphological

properties of a particular ferrite (Co0.5Zn0.5Fe2O4) to be prepared by mechanical

alloying.

1.2 Ferrite materials

In recent years, there has been considerable interest in the study of properties of

nanosized ferrite particles because of the importance in the fundamental

understanding of the physics of the properties as well as their proposed applications

for many technological purposes (Sharma et al., 2005). For example, these

applications include high frequency (HF) choke filters, HF transformer, antenna rods,

etc. (Moulson and Herbert, 1990).

Generally, the mixed oxides containing iron oxides as their main component are

called ferrite materials. Unlike most materials, they possess both high permeability

and moderate permittivity at frequencies from direct current (DC) to the millimeter

wavelengths (Harris et al., 2009).

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In commercial industry, ferrites materials can be classified in three important types,

each one having a specific crystal structure listed below:

a) Spinel ferrites, for example NiZn-, MnZn- and MgMnZn ferrite.

b) Garnet structure microwave ferrites, for example Yitrium iron garnet

c) Magnetoplumbite (Hexagonal) ferrites, for example Barium (Ba) and Sr

hexaferrites

In general, types a) and b) can be grouped in one group of “soft” ferrites, while type

c) can be grouped into “hard” ferrites. The terms of “soft” and “hard” refer to the

characteristics and properties of the ferrites. The “soft” ferrites means that it‟s easy to

magnetise and easy to dimagnetise the ferrite materials; meanwhile, the “hard”

ferrites are difficult to magnetise and also difficult to dimagnetise.

In the present work, the only interest on the soft ferrite and are just focused on the

spinel ferrites (type a).

1.3 Problem Statement

Many researchers just focused on the sintering and synthesis to get the better material

in the studies of spinel ferrites. However, what would be the composition-

microstructure relationship at the various intermediate sintering conditions during the

parallel evolutions of the morphology and the materials properties? After more than

eight decades of ferrite research, this question has been hardly answered. Hence it is

now taken as the problem statement of this research work with specific form an the

Co0.5Zn0.5Fe2O4 ferrite

1.4 Objectives

The ultimate goals of this research to determine the relationship between magnetic

properties and microstructure parameter which exists during any states of their

parallel evolution and to explain the underlying science for their relationship, it is

interesting to study the evolution of the magnetic properties starting with and from

nano material powder. However, to achieve the goals above, the necessary work has

to be carried out and these research-work steps have the following objectives:

1. To prepare Co0.5Zn0.5Fe2O4 using mechanically alloyed nanoparticles

2. To study the phase formation of the as-prepared ferrite using X-ray

diffraction (XRD)

3. To study the effect of the sintering temperature on the microstructure

evolution and magnetic properties

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1.5 Thesis outline

This thesis consists of six chapters. First chapter introduces the ferrite material, the

problem statement and the objectives of this research. Chapter two is devoted to the

literature review on preparation of ferrite, structure of spinel ferrite and application

of the theory that will be used for this research. The Methodology of this research is

presented in Chapter three. Meanwhile, results and discussion are covered in Chapter

four. Finally Chapter five provides the summary of this research and suggestions for

future work.

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BIBLIOGRAPHY

Azadmanjiri, J. (2008). Structural and electromagnetic properties of Ni–Zn ferrites

prepared by sol–gel combustion method. Materials Chemistry and Physics,

109(1), 109-112. doi:10.1016/j.matchemphys.2007.11.001

Bean, C. P. (1955). Hysteresis Loops of Mixtures of Ferromagnetic Micropowders.

Journal of Applied Physics, 26(11), 1381-1383.

Bas, J. A., Calero, J. A., and Dougan, M. J. (2003). Sintered soft magnetic materials .

Properties and applications, Journal of Magnetism and Magnetic Materials,

255, 391-398.

Coble, R.L. (1961). Sintering crystalline solids. I. intermediate and final state

diffusion models, J. Appl. Phys. 32, 787-792.

Gul, I. H., Abbasi, a. Z., Amin, F., Anis-ur-Rehman, M., & Maqsood, a. (2007).

Structural, magnetic and electrical properties of Co1−xZnxFe2O4 synthesized by

co-precipitation method. Journal of Magnetism and Magnetic Materials, 311(2),

494-499

Goldman, A. (1990). Modern Ferrite Technology, second ed. Springer, Pittsburg,

PA, USA.

Goldman A., (1999) Handbook of Modern Ferromagnetic Materials, Kluwer

Academic Publishers.

Goldman, A. (2006). Modern Ferrite Technology (2nd ed.). Pittsburgh: Springer

Science and Business Media, Inc.

Guillaud,C., Paulus, M. (1956). Handbook of Modern Ferromagnetic Materials. In A.

Goldman (Ed.), Handbook of Modern Ferromagnetic Materials.

Massachusetts: Kluwer Academic Publihers.

Han, Z., Li, D., Liu, X., Geng, D., Li, J., & Zhang, Z. (2009). Microwave-absorption

properties of Fe(Mn)/ferrite nanocapsules. Journal of Physics D: Applied

Physics, 42(5), 055008.

Harris, V. G., Geiler, A., Chen, Y., Yoon, S. D., Wu, M., Yang, A., Chen, Z., et al.

(2009). Recent advances in processing and applications of microwave ferrites.

Journal of Magnetism and Magnetic Materials, 321(14), 2035-2047.

Halliday, D., Resnick, R., and Walker, J. (1997). Fundamentals of Physics

(Extended, 5th ed ed.). New York: Wiley & Sons, Inc.

© COPYRIG

HT UPM

59

Ismail, I., and Hashim, M. (2012). Sintering Temperature Dependence of Evolving

Morphologies and Magnetic Properties of Ni0.5Zn0.5Fe2O4 Synthesized via

Mechanical alloying. Journal of Superconductivity and Novel Magnetism, 25(5),

1551-1561.

Ishino, K., and Narumiya, Y. (1987). Development of magnetic ferrites: control and

application of losses. American Ceramic Society Bulletin, 66(10), 1469- 1474

Jahanbin, T., Hashim, M., and Amin Matori, K. (2010). Comparative studies on the

structure and electromagnetic properties of Ni−Zn ferrites prepared via co-

precipitation and conventional ceramic processing routes. Journal of Magnetism

and Magnetic Materials, 322(18), 2684-2689. Elsevier

Jarcho, M., Bolen, C.H., Thomas, M.B., Bobick, J., Kay, J.K., Doremus, R.H.

(1976). Hydroxylapatite synthesis and characterization in dense polycrystalline

form, J. Mater Sci 11, 2027-2035.

Jiang, X., Trunov, M. a., Schoenitz, M., Dave, R. N., & Dreizin, E. L. (2009).

Mechanical alloying and reactive milling in a high energy planetary mill.

Journal of Alloys and Compounds, 478(1-2), 246-251.

Khan, H. M. (2011). Electrical Transport Properties of Bi2O3-Doped CoFe2O4 and

CoHo0.02Fe1.98O4 Ferrites. Materials Sciences and Applications, 02(08), 1083-

1089.

Kingery, W.D., Bowen, H.K. and Uhlmann, D.R. (1976). Introduction to Ceramics

(2nd edition). John Wiley & Sons, New York.

Köseoğlu, Y., Baykal, a., Gözüak, F., and Kavas, H. (2009). Structural and magnetic

properties of CoxZn1−xFe2O4 nanocrystals synthesized by microwave method.

Polyhedron, 28(14), 2887-2892.

Liu, Y., Zhu, X.-guang, Zhang, L., Min, F.-fei, & Zhang, M.-xu. (2012).

Microstructure and magnetic properties of nanocrystalline Co1−xZnxFe2O4

ferrites. Materials Research Bulletin, 47(12), 4174-4180. Elsevier Ltd.

Mathew, D. S., and Juang, R.-S. (2007). An overview of the structure and

magnetism of spinel ferrite nanoparticles and their synthesis in microemulsions.

Chemical Engineering Journal, 129(1-3), 51-65.

Mott, N. F. (1968). 1. The model for hopping conduction in glasses,journal of non-

crystalline solids 1,1-17.

Moulson, A. J., Herbert, J. M. (1990). Electroceramics: Materials, Properties and

Applications (2nd ed.). London: Chapman & Hall

Pal, M., and Chakravorty, D. (2003). Nanocrystalline magnetic alloys and ceramics,

28(April), 283-297.

© COPYRIG

HT UPM

60

Pandya, P. B., Joshi, H. H., and Kulkarni, R. G. (1991). Bulk magnetic properties of

Co-Zn ferrites prepared by the co-precipitation method. Journal of Materials

Science, 26(20), 5509-5512.

P. Sandra. (2011). Sintering and Microstructure. Ceramics , 1-15.

Qu, Y., Yang, H., Yang, N., Fan, Y., Zhu, H., and Zou, G. (2006). The effect of

reaction temperature on the particle size, structure and magnetic properties of

coprecipitated CoFe2O4 nanoparticles. Materials Letters, 60(29-30), 3548-3552.

Rao, A. D. P., Ramesh, B., Rao, P. R. M., Raju, S. B. (1999). Magnetic and

microstructural properties of Sn/Nb substituted Mn–Zn ferrites Journal of

Alloys and Compounds, 282(1-2), 268-273.

Sanchez, Rivas, J., Vaqueiro, P., & Caeiro, D. (2002). Particle size effects on

magnetic properties of yttrium iron garnets prepared by a sol – gel method, 247,

92-98.

Sharma, R. K., Suwalka, O., Lakshmi, N., Venugopalan, K., Banerjee, a., and Joy, P.

a. (2005). Synthesis of chromium substituted nano particles of cobalt zinc

ferrites by coprecipitation. Materials Letters, 59(27), 3402-3405.

Sharifi, I., and Shokrollahi, H. (2012). Nanostructural, magnetic and Mössbauer

studies of nanosized Co1−xZnxFe2O4 synthesized by co-precipitation. Journal of

Magnetism and Magnetic Materials, 324(15), 2397-2403.

Shinde, T.J. Gadkari, A.B. and Vasambekar, P.N. (2008). DC resistivity of Ni-Zn

ferrites prepared by oxalate precipitation method. Mater. Chem. Phy. 111(1), 87-

91.

Shackelford. J.F. (2000). Introduction to materials science for engineers (fifth

edition). Prentice Hall International, Inc. New Jersey.

Singhal, S. (2010). Effect of Zn Substitution on the Magnetic Properties of Cobalt

Ferrite Nano Particles Prepared Via Sol-Gel Route. Journal of Electromagnetic

Analysis and Applications, 02(06), 376-381.

Snelling, E.C., (1969). Soft Ferrites: Properties and applications, 1st Edition, Iliffe

Books Ltd, London

Sun, K., Ian, Z., Chen, S., Sun, Y., Yu, Z., (2006). Effect of sintering process on

microstructure and magnetic properties of high frequency power ferrite, Rare

Metals, 25, 509-514.

Suryanarayana, C., Ivanov, E., and Boldyrev, V. (2001). The science and technology

of mechanical alloying. Materials Science and Engineering: A, 304-306, 151-

158

© COPYRIG

HT UPM

61

Thakur, A., and Chevalier, A. (2009). Low-loss Magnetodielectric Spinel-ferrite

Based Ceramic with Constant Permeability and Permittivity in the UHF Range,

1-5.

Waje, S. B., Hashim, M., Wan Yusoff, W. D., and Abbas, Z. (2010). Sintering

temperature dependence of room temperature magnetic and dielectric properties

of Co0.5Zn0.5Fe2O4 prepared using mechanically alloyed nanoparticles. Journal

of Magnetism and Magnetic Materials, 322(6), 686-691. Elsevier.

Vaidyanathan, G., Sendhilnathan, S., and Arulmurugan, R. (2007). Structural and

magnetic properties of Co1−xZnxFe2O4 nanoparticles by co-precipitation method.

Journal of Magnetism and Magnetic Materials, 313(2), 293-299.

Viswanathan, B. and Murthy, V.R.K., (1990). Ferrite Materials: Science and

Technology, Narosa Publishing House.